WO2011104996A1 - Thermosetting resin composition, b-stage thermally conductive sheet, and power module - Google Patents
Thermosetting resin composition, b-stage thermally conductive sheet, and power module Download PDFInfo
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- WO2011104996A1 WO2011104996A1 PCT/JP2010/073776 JP2010073776W WO2011104996A1 WO 2011104996 A1 WO2011104996 A1 WO 2011104996A1 JP 2010073776 W JP2010073776 W JP 2010073776W WO 2011104996 A1 WO2011104996 A1 WO 2011104996A1
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Abstract
Description
また、本発明は、電気絶縁性及び熱放散性に優れたパワーモジュールを提供することを目的とする。 The present invention has been made in order to solve the above-described problems, and has excellent thermal conductivity while maintaining electrical insulation by controlling the occurrence location and size of defects such as voids and cracks. It aims at obtaining the thermosetting resin composition which gives the heat conductive sheet which has, and a B-stage heat conductive sheet.
Moreover, an object of this invention is to provide the power module excellent in electrical insulation and heat dissipation.
すなわち、本発明は、無機充填材及び熱硬化性樹脂マトリックス成分を含む熱硬化性樹脂組成物であって、前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有することを特徴とする熱硬化性樹脂組成物である。 As a result of diligent research to solve the above problems, the present inventors incorporated secondary sintered particles having voids of a specific size, thereby secondary generation of defects due to deformation relaxation. It was found that the generation of large defects in the base portion (thermosetting resin matrix between the inorganic fillers) of the heat conductive sheet can be suppressed by restricting the voids in the particles and controlling the size of the defects.
That is, the present invention is a thermosetting resin composition comprising an inorganic filler and a thermosetting resin matrix component, wherein the inorganic filler is a secondary sintered particle composed of primary particles of scaly boron nitride. And at least a part of the secondary sintered particles has a maximum void diameter of 5 μm or more and 80 μm or less.
さらに、本発明は、無機充填材を熱硬化性樹脂マトリックス中に分散してなる熱伝導性シートであって、前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有する熱伝導性シートを具備することを特徴とするパワーモジュールである。 Further, the present invention is a B-stage heat conductive sheet obtained by dispersing an inorganic filler in a thermosetting resin matrix in a B-stage state, and the inorganic filler is composed of primary particles of scaly boron nitride. The B-stage heat conductive sheet is characterized in that the secondary sintered particles are included and at least a part of the secondary sintered particles has a maximum void diameter of 5 μm or more and 80 μm or less.
Furthermore, the present invention is a thermally conductive sheet in which an inorganic filler is dispersed in a thermosetting resin matrix, and the inorganic filler is secondary sintered composed of primary particles of scaly boron nitride. A power module comprising a thermally conductive sheet containing particles and at least a part of the secondary sintered particles having a maximum void diameter of 5 μm or more and 80 μm or less.
また、本発明によれば、電気絶縁性及び熱放散性に優れたパワーモジュールを提供することができる。 According to the present invention, a thermosetting resin composition that provides a thermally conductive sheet having excellent thermal conductivity while maintaining electrical insulation by controlling the occurrence location and size of defects such as voids and cracks, and A B-stage heat conductive sheet can be obtained.
Moreover, according to this invention, the power module excellent in electrical insulation and heat dissipation can be provided.
本実施の形態の熱硬化性樹脂組成物は、無機充填材及び熱硬化性樹脂マトリックス成分を含む。
本実施の形態の熱硬化性樹脂組成物に用いられる無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含む。本明細書において「二次焼結粒子」は、鱗片状窒化ホウ素の一次粒子を凝集して焼結させたものを意味し、当該技術分野において一般的に公知である。しかしながら、一般的な二次焼結粒子は、鱗片状窒化ホウ素の一次粒子の間に形成された小さな空隙(具体的には0.5μm未満の最大空隙径を有する空隙)をもつのに対し、本実施の形態の熱硬化性樹脂組成物に用いられる二次焼結粒子の少なくとも一部は、5μm以上80μm以下の最大空隙径を有する空隙をもつ。本実施の形態の熱硬化性樹脂組成物は、このような最大空隙径を有する二次焼結粒子を配合することにより、熱伝導性シートにおける欠陥の発生箇所及び大きさを適切に制御することができる。最大空隙径が5μm未満であると、熱伝導性シートのベース部分に発生する欠陥を抑制することができず、熱伝導性シートの電気絶縁性が低下する。一方、最大空隙径が80μmを超えると、熱伝導性シートのベース部分に発生する欠陥については抑制することができるものの、二次焼結粒子の空隙内に発生する欠陥が大きくなりすぎてしまい、熱伝導性シートの電気絶縁性が低下する。
The thermosetting resin composition of the present embodiment includes an inorganic filler and a thermosetting resin matrix component.
The inorganic filler used in the thermosetting resin composition of the present embodiment includes secondary sintered particles composed of primary particles of scaly boron nitride. In the present specification, “secondary sintered particles” mean particles obtained by agglomerating and sintering primary particles of scaly boron nitride, and are generally known in the art. However, while general secondary sintered particles have small voids (specifically voids having a maximum void diameter of less than 0.5 μm) formed between the primary particles of scaly boron nitride, At least a part of the secondary sintered particles used in the thermosetting resin composition of the present embodiment has a void having a maximum void diameter of 5 μm or more and 80 μm or less. The thermosetting resin composition of the present embodiment appropriately controls the location and size of defects in the heat conductive sheet by blending secondary sintered particles having such a maximum void diameter. Can do. If the maximum gap diameter is less than 5 μm, defects generated in the base portion of the thermally conductive sheet cannot be suppressed, and the electrical insulation of the thermally conductive sheet is deteriorated. On the other hand, when the maximum void diameter exceeds 80 μm, defects that occur in the base portion of the heat conductive sheet can be suppressed, but defects generated in the voids of the secondary sintered particles become too large, The electrical insulation property of the heat conductive sheet is lowered.
以下、本明細書において、0.5μm未満の最大空隙径を有する空隙をもつ二次焼結粒子を「中実二次焼結粒子」、0.5μm以上の最大空隙径を有する空隙をもつ二次焼結粒子を「中空二次焼結粒子」、中実二次焼結粒子及び中空二次焼結粒子の両方を「二次焼結粒子」という。 Here, in this specification, the “maximum void diameter of secondary sintered particles” means that a thermally conductive sheet in which secondary sintered particles are dispersed in a thermosetting resin matrix is actually produced, and this heat conduction is achieved. It means a value obtained by actually measuring the maximum diameter of the voids of the secondary sintered particles after taking several photos of the cross-section of the conductive sheet that have been magnified several thousand times with an electron microscope.
Hereinafter, in this specification, secondary sintered particles having voids having a maximum void diameter of less than 0.5 μm are referred to as “solid secondary sintered particles”, and those having voids having a maximum void diameter of 0.5 μm or more. The secondary sintered particles are referred to as “hollow secondary sintered particles”, and both the solid secondary sintered particles and the hollow secondary sintered particles are referred to as “secondary sintered particles”.
この中空二次焼結粒子1の最大空隙径は、中空二次焼結粒子1の平均粒径の2/3以下であることが好ましい。中空二次焼結粒子1の最大空隙径が、中空二次焼結粒子1の平均粒径の2/3を超えると、大きな空隙3周りの殻の部分が薄くなりすぎてしまい、加圧工程の際(例えば、Bステージ熱伝導性シートを作製する際の圧力や、パワーモジュールを作製する際のトランスファモールド成形圧力)に、大きな空隙3を維持できないことがある。 Here, a cross-sectional view of the hollow secondary sintered particles is shown in FIG. As shown in FIG. 1, the hollow secondary
The maximum void diameter of the hollow secondary sintered
h=2Tcosθ/ρgr (1)
上記式(1)中、hは熱硬化性樹脂マトリックスの流出し易さ(m)を表し、Tは表面張力(N/m)を表し、θは接触角(°)を表し、ρは熱硬化性樹脂マトリックスの密度(kg/m3)を表し、gは重力加速度(m/m2)を表し、rは熱伝導性シートのベース部分に発生する欠陥の径及び中空二次焼結粒子1の最大空隙径(m)を表す。
この式(1)からわかるように、熱硬化性樹脂マトリックスが溶融した際の熱硬化性樹脂マトリックスの流出し易さは、熱伝導性シートのベース部分に発生する欠陥の径や、中空二次焼結粒子1の最大空隙径と関係しており、これらの径が小さいものほど毛細管力が大きいといえる。つまり、熱伝導性シートのベース部分に発生する欠陥の径よりも中空二次焼結粒子1の最大空隙径を大きくすることで、溶融した熱硬化性樹脂マトリックスの流動性を制御することができる。 Here, the capillary phenomenon when the B stage heat conductive sheet is exposed to a high temperature in a non-pressurized state and the thermosetting resin matrix melts and flows is generally expressed by the following equation (1). Can do.
h = 2T cos θ / ρgr (1)
In the above formula (1), h represents the ease of outflow of the thermosetting resin matrix (m), T represents the surface tension (N / m), θ represents the contact angle (°), and ρ represents heat. Represents the density (kg / m 3 ) of the curable resin matrix, g represents the acceleration of gravity (m / m 2 ), r represents the diameter of defects generated in the base portion of the heat conductive sheet and the hollow secondary
As can be seen from this equation (1), the easiness of the flow of the thermosetting resin matrix when the thermosetting resin matrix is melted depends on the diameter of defects generated in the base portion of the heat conductive sheet, the hollow secondary This is related to the maximum void diameter of the
他方、中空二次焼結粒子1を含まない熱硬化性樹脂組成物から得られる熱伝導性シートの断面図を図3に示す。図3において、熱伝導性シートは、熱硬化性樹脂マトリックス5と、熱硬化性樹脂マトリックス5中に分散された中実二次焼結粒子4及び下記で説明する任意の鱗片状窒化ホウ素の一次粒子6とから構成されている。この熱伝導性シートでは、ベース部分(無機充填材間の熱硬化性樹脂マトリックス5部分)に発生する空隙を制御することができないために大きな欠陥7が発生し、電気絶縁性が低下する。 Next, FIG. 2 shows a cross-sectional view of a heat conductive sheet obtained from the thermosetting resin composition of the present embodiment. In FIG. 2, the heat conductive sheet includes a
On the other hand, FIG. 3 shows a cross-sectional view of a heat conductive sheet obtained from a thermosetting resin composition that does not contain the hollow secondary
なお、二次焼結粒子の形状は、球状に限定されず、鱗片状などの他の形状であってもよい。ただし、球状以外の他の形状の場合、平均粒径は当該形状における長辺の長さを意味する。また、球状の二次焼結粒子であれば、熱硬化性樹脂組成物を製造する際に、熱硬化性樹脂マトリックス成分の流動性を確保しつつ、二次焼結粒子の配合量を高めることができるため、二次焼結粒子は球状であることが好ましい。 Further, if the maximum particle size of the secondary sintered particles is too large with respect to the thickness of the heat conductive sheet, there is a possibility that the electrical insulation properties may be lowered through the interface. Accordingly, the maximum particle size of the secondary sintered particles is preferably about 90% or less of the thickness of the heat conductive sheet.
The shape of the secondary sintered particles is not limited to a spherical shape, and may be another shape such as a scale shape. However, in the case of a shape other than the spherical shape, the average particle diameter means the length of the long side in the shape. In addition, when the spherical secondary sintered particles are used, when the thermosetting resin composition is produced, the blending amount of the secondary sintered particles is increased while ensuring the fluidity of the thermosetting resin matrix component. Therefore, the secondary sintered particles are preferably spherical.
上記のようにして形成された中空二次凝集粒子及び中実二次凝集粒子は、焼結させることにより、それぞれ中空二次焼結粒子1及び中実二次焼結粒子4とすることができる。 Specifically, the solid secondary agglomerated particles are spray-dried using a slurry containing 30 parts by mass or more and 120 parts by mass or less of water with respect to 100 parts by mass of the scaly boron nitride
The hollow secondary agglomerated particles and the solid secondary agglomerated particles formed as described above can be made into the hollow secondary
熱硬化性樹脂としては、特に限定されず、当該技術分野において公知のものを用いることができる。熱硬化性樹脂の例としては、エポキシ樹脂、不飽和ポリエステル樹脂、フェノール樹脂、メラミン樹脂、シリコーン樹脂、ポリイミド樹脂などが挙げられる。
また、熱硬化性樹脂は、耐熱性に優れた熱伝導性シートを得る観点から、耐熱性に優れた熱硬化性樹脂マトリックス5を与えるものであることが好ましい。具体的には、180℃~250℃の温度に曝されても本来の物性を失わない熱硬化性樹脂マトリックス5を与える熱硬化性樹脂であることが好ましい。このような熱硬化性の例としては、耐熱性エポキシ樹脂が挙げられる。耐熱性エポキシ樹脂は、1分子中に2個以上のエポキシ基を有し、好ましくは100以上1000以下、より好ましくは150以上500の範囲のエポキシ当量を有するものが望ましい。 The thermosetting resin matrix component used for the thermosetting resin composition of this Embodiment is a component which provides the
It does not specifically limit as a thermosetting resin, A well-known thing can be used in the said technical field. Examples of the thermosetting resin include an epoxy resin, an unsaturated polyester resin, a phenol resin, a melamine resin, a silicone resin, and a polyimide resin.
Moreover, it is preferable that a thermosetting resin gives the
熱硬化性樹脂組成物における硬化剤の配合量は、使用する熱硬化性樹脂や硬化剤の種類などに応じて適宜調整すればよく、一般的に、100質量部の熱硬化性樹脂に対して0.1質量部以上200質量部以下である。 It does not specifically limit as a hardening | curing agent, What is necessary is just to select a well-known thing suitably according to the kind of thermosetting resin to be used. In particular, when an epoxy resin is used as the thermosetting resin, examples of the curing agent include alicyclic acid anhydrides such as methyltetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, and hymic anhydride; dodecenyl succinic anhydride, etc. Aliphatic anhydrides; aromatic anhydrides such as phthalic anhydride and trimellitic anhydride; organic dihydrazides such as dicyandiamide and adipic dihydrazide; tris (dimethylaminomethyl) phenol; dimethylbenzylamine; 1,8-diazabicyclo (5,4,0) undecene and derivatives thereof; imidazoles such as 2-methylimidazole, 2-ethyl-4-methylimidazole and 2-phenylimidazole; phenol novolak, o-cresol novolak, p-cresol novolak, t- Butylpheno Lunovolak, dicyclopentadiene cresol, polyparavinylphenol, bisphenol A type novolak, xylylene modified novolak, decalin modified novolak, poly (di-o-hydroxyphenyl) methane, poly (di-m-hydroxyphenyl) methane, poly (di Phenolic resins such as -p-hydroxyphenyl) methane. These can be used alone or in combination of two or more.
What is necessary is just to adjust suitably the compounding quantity of the hardening | curing agent in a thermosetting resin composition according to the kind of thermosetting resin to be used, a hardening agent, etc., and generally with respect to 100 mass parts thermosetting resin. It is 0.1 mass part or more and 200 mass parts or less.
そこで、上記の問題を解決するために、本実施の形態の熱硬化性樹脂組成物は、特定の密着性付与剤を特定の割合で含むことが好ましい。この密着性付与剤を配合することによって、二次焼結粒子の空隙に密着性付与剤と共に熱硬化性樹脂マトリックス成分を浸透させ易くすると共に、ハンドリング性を低下させることなく、熱硬化性樹脂マトリックス5と二次焼結粒子との間の密着性を高めた熱伝導シートを得ることが可能になる。 Since the
Therefore, in order to solve the above problem, the thermosetting resin composition of the present embodiment preferably contains a specific adhesion-imparting agent at a specific ratio. By blending this adhesion-imparting agent, the thermosetting resin matrix component can be easily penetrated into the voids of the secondary sintered particles together with the adhesion-imparting agent, and the handling property is not lowered. It becomes possible to obtain the heat conductive sheet which improved the adhesiveness between 5 and secondary sintered particle.
上記一般式(1)で表されるビスフェノール型エポキシ樹脂は、一般に市販されており、例えば、ジャパンエポキシレジン株式会社から販売されているJER E1256、E4250、E4275などを用いることができる。 , Preferably a bisphenol A skeleton, a bisphenol F skeleton or a bisphenol A / F mixed skeleton, B is CH 2 , CH (CH 3 ) or C (CH 3 ) 2 , and n is 0 to 10, preferably Is 1-8. Here, the bisphenol A / F mixed skeleton means a skeleton having both a bisphenol A skeleton and a bisphenol F skeleton.
The bisphenol type epoxy resin represented by the general formula (1) is generally commercially available, and for example, JER E1256, E4250, E4275, etc. sold by Japan Epoxy Resin Co., Ltd. can be used.
上記一般式(2)で表されるアルキレンオキサイド変性ビスフェノール型エポキシ樹脂は、一般に市販されており、例えば、ジャパンエポキシレジン株式会社から販売されているYL7175-500、YL7175-1000や、DIC株式会社から販売されているEPICLON EXA4850、4816、4822などを用いることができる。 In the above formula (2), B is CH 2 , CH (CH 3 ) or C (CH 3 ) 2 , X is an ethyleneoxyethyl group, a di (ethyleneoxy) ethyl group, a tri (ethyleneoxy) ethyl group, Tetra (ethyleneoxy) ethyl group, propyleneoxypropyl group, di (propyleneoxy) propyl group, tri (propyleneoxy) propyl group, tetra (propyleneoxy) propyl group, butyleneoxybutyl group, di (butyleneoxy) butyl group, A tri (butyleneoxy) butyl group, a tetra (butyleneoxy) butyl group, an alkylene group having 2 to 15 carbon atoms, or an aliphatic hydrocarbon group having 6 to 17 carbon atoms having a cycloalkane skeleton, and m is 0 -20, preferably 2-5.
The alkylene oxide-modified bisphenol-type epoxy resin represented by the general formula (2) is generally commercially available. For example, YL7175-500, YL7175-1000 sold by Japan Epoxy Resin Co., Ltd., and DIC Corporation. EPICLON EXA 4850, 4816, 4822, etc. which are sold can be used.
スチレン系ポリマーの中でも、エポキシ基を有するスチレン系ポリマーが好ましい。このようなスチレン系ポリマーは、一般に市販されており、例えば、日油株式会社から販売されているマープルーフ(登録商標)G-0115S、G-0250S、G-1005SAなどを用いることができる。 The styrenic polymer means a polymer having a styrene unit in the molecular chain. For example, polystyrene, styrene-methyl methacrylate copolymer, acrylonitrile-styrene copolymer, maleic anhydride-styrene copolymer, maleimide- Examples thereof include styrene copolymers and acrylonitrile-hudadiene-styrene.
Among styrene polymers, styrene polymers having an epoxy group are preferable. Such styrenic polymers are generally commercially available, and, for example, Marproof (registered trademark) G-0115S, G-0250S, G-1005SA and the like sold by NOF Corporation can be used.
カップリング剤の配合量は、使用する熱硬化性樹脂やカップリング剤の種類などにあわせて適宜設定すればよいが、一般的に、100質量部の熱硬化性樹脂に対して0.01質量部以上5質量部以下である。 The thermosetting resin composition of this Embodiment can contain a coupling agent from a viewpoint of improving the adhesive force of the interface of the
The blending amount of the coupling agent may be appropriately set according to the type of thermosetting resin or coupling agent to be used, but generally 0.01 mass with respect to 100 parts by mass of the thermosetting resin. Part to 5 parts by mass.
熱硬化性樹脂組成物における溶剤の配合量は、混練が可能な量であれば特に限定されず、一般的に、熱硬化性樹脂と無機充填剤との合計100質量部に対して40質量部以上300質量部以下である。 The thermosetting resin composition of the present embodiment can further contain a solvent from the viewpoint of adjusting the viscosity of the composition. It does not specifically limit as a solvent, What is necessary is just to select a well-known thing suitably according to the kind of thermosetting resin and inorganic filler to be used. Examples of such solvents include toluene and methyl ethyl ketone. These can be used alone or in combination of two or more.
The amount of the solvent in the thermosetting resin composition is not particularly limited as long as kneading is possible, and generally 40 parts by mass with respect to 100 parts by mass in total of the thermosetting resin and the inorganic filler. The amount is 300 parts by mass or less.
まず、所定量の熱硬化性樹脂、この熱硬化性樹脂を硬化させるために必要な量の硬化剤、及び必要であれば所定量の密着性付与剤8を混合する。
次に、この混合物に溶剤を加えた後、二次焼結粒子などの無機充填材を加えて予備混合する。なお、混合物の粘度が低い場合には、溶剤を加えなくてもよい。
次に、この予備混合物を3本ロールやニーダなどを用いて混練することによって熱硬化性樹脂組成物を得ることができる。なお、熱硬化性樹脂組成物にカップリング剤を配合する場合、カップリング剤は混練工程前までに加えればよい。 The manufacturing method of the thermosetting resin composition of this Embodiment containing the above structural components is not specifically limited, It can carry out according to a well-known method. For example, the thermosetting resin composition of the present embodiment can be manufactured as follows.
First, a predetermined amount of thermosetting resin, a necessary amount of curing agent for curing the thermosetting resin, and a predetermined amount of adhesion-imparting
Next, after adding a solvent to this mixture, an inorganic filler such as secondary sintered particles is added and premixed. In addition, when the viscosity of a mixture is low, it is not necessary to add a solvent.
Next, a thermosetting resin composition can be obtained by kneading the preliminary mixture using a three roll or a kneader. In addition, what is necessary is just to add a coupling agent before a kneading | mixing process, when mix | blending a coupling agent with a thermosetting resin composition.
本実施の形態のBステージ熱伝導性シートは、上記の熱硬化性樹脂組成物をシート化して半硬化させたものである。すなわち、本実施の形態のBステージ熱伝導性シートは、無機充填材をBステージ状態の熱硬化性樹脂マトリックス中に分散してなるBステージ熱伝導性シートであって、前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有することを特徴とする。
The B-stage heat conductive sheet of the present embodiment is a sheet obtained by semi-curing the thermosetting resin composition described above. That is, the B-stage heat conductive sheet of the present embodiment is a B-stage heat conductive sheet in which an inorganic filler is dispersed in a thermosetting resin matrix in a B-stage state, and the inorganic filler is It includes secondary sintered particles composed of primary particles of flaky boron nitride, and at least a part of the secondary sintered particles has a maximum void diameter of 5 μm or more and 80 μm or less.
ここで、基材としては、特に限定されず、例えば、離型処理された樹脂シートやフィルムなどのような公知の基材を用いることができる。また、基材として銅箔などの金属板を用い、金属板付のBステージ熱伝導性シートとしてもよい。
熱硬化性樹脂組成物の塗布方法としては、特に限定されず、ドクターブレード法などのような公知の方法を用いることができる。
塗布した熱硬化性樹脂組成物の乾燥は、周囲温度で行ってよいが、溶剤の揮発を促進させる観点から、必要に応じて80℃以上150℃以下に加熱してもよい。 The B-stage heat conductive sheet of the present embodiment can be produced by a method including a step of applying the thermosetting resin composition to a substrate and drying the substrate, and a step of semi-curing the applied dried product. it can.
Here, it does not specifically limit as a base material, For example, well-known base materials, such as a resin sheet and a film by which the mold release process was carried out, can be used. Moreover, it is good also as a B-stage heat conductive sheet with a metal plate, using metal plates, such as copper foil, as a base material.
The method for applying the thermosetting resin composition is not particularly limited, and a known method such as a doctor blade method can be used.
The applied thermosetting resin composition may be dried at ambient temperature, but may be heated to 80 ° C. or higher and 150 ° C. or lower as needed from the viewpoint of promoting the volatilization of the solvent.
また、塗布乾燥物を半硬化させる場合、必要に応じて加圧してもよい。特に、上記の乾燥工程によって塗布乾燥物内に欠陥が発生した場合には、加圧して欠陥を除去しておくことが好ましい。この場合のプレス圧は、好ましくは0.5MPa以上30MPa以下、より好ましくは4MPa以上20MPa以下、最も好ましくは4MPa以上15MPa以下である。プレス圧が0.5MPa未満であると、Bステージ熱伝導性シート内の欠陥を十分に除去することができないことがある。一方、プレス圧が30MPaを超えると、二次焼結粒子が変形又は崩壊してしまい、熱伝導性シートの熱伝導性及び電気絶縁性が低下することがある。また、プレス時間は、特に限定されないが、一般的に5分以上60分以下である。 The semi-curing temperature of the coated and dried product may be appropriately set according to the type of thermosetting resin to be used, but is generally 80 ° C. or higher and 200 ° C. or lower. The semi-curing time is not particularly limited, but is generally 2 minutes or longer and 24 hours or shorter.
Moreover, when semi-curing the coated dried product, it may be pressurized as necessary. In particular, when a defect occurs in the dried product by the above drying process, it is preferable to press the pressure to remove the defect. The pressing pressure in this case is preferably 0.5 MPa or more and 30 MPa or less, more preferably 4 MPa or more and 20 MPa or less, and most preferably 4 MPa or more and 15 MPa or less. If the press pressure is less than 0.5 MPa, defects in the B-stage thermally conductive sheet may not be sufficiently removed. On the other hand, when the press pressure exceeds 30 MPa, the secondary sintered particles are deformed or collapsed, and the thermal conductivity and electrical insulation of the thermal conductive sheet may be lowered. The pressing time is not particularly limited, but is generally 5 minutes or more and 60 minutes or less.
本実施の形態のパワーモジュールは、上記の熱硬化性樹脂組成物又はBステージ熱伝導性シートから得られる熱伝導性シートを具備する。すなわち、本実施の形態のパワーモジュールは、無機充填材を熱硬化性樹脂マトリックス中に分散してなる熱伝導性シートであって、前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有する熱伝導性シートを具備することを特徴とする。
本実施の形態のパワーモジュールにおいて、熱伝導性シート以外の構成は特に限定されず、公知のパワーモジュールの構成を採用することができる。
The power module of the present embodiment includes a heat conductive sheet obtained from the thermosetting resin composition or the B-stage heat conductive sheet. That is, the power module of the present embodiment is a thermally conductive sheet in which an inorganic filler is dispersed in a thermosetting resin matrix, and the inorganic filler is composed of primary particles of scaly boron nitride. And at least a part of the secondary sintered particles include a thermally conductive sheet having a maximum void diameter of 5 μm or more and 80 μm or less.
In the power module of the present embodiment, the configuration other than the heat conductive sheet is not particularly limited, and a known power module configuration can be adopted.
図6は、本実施の形態のパワーモジュールの断面図である。図6において、パワーモジュールは、熱伝導性シート11と、熱伝導性シート11を狭持するヒートシンク10及びリードフレーム12と、リードフレーム12上に搭載された電力半導体素子13とを備えている。そして、電力半導体素子13の間、及び電力半導体素子13とリードフレーム12との間は、金属線14によってワイヤボンディングされている。また、リードフレーム12の外部接続用端部、及びヒートシンク10の外部放熱部以外は封止樹脂15で封止されている。 Hereinafter, an example of the power module of the present embodiment will be described with reference to the drawings.
FIG. 6 is a cross-sectional view of the power module of the present embodiment. In FIG. 6, the power module includes a heat
ワイドバンドギャップ半導体によって形成された電力半導体素子13は、耐電圧性が高く、許容電流密度も高いため、電力半導体素子13の小型化が可能となる。そして、このように小型化された電力半導体素子13を用いることにより、電力半導体素子13を組み込んだパワーモジュールの小型化も可能になる。
また、ワイドバンドギャップ半導体により形成された電力半導体素子13は、耐熱性も高いため、ヒートシンク10、熱伝導性シート11、リードフレーム12などの小型化にもつながり、パワーモジュールの一層の小型化が可能になる。
さらに、ワイドバンドギャップ半導体により形成された電力半導体素子13は、電力損失も低いため、素子としての高効率化も可能となる。 In this power module, members other than the heat
Since the
In addition, since the
Furthermore, since the
図7は、本実施の形態のパワーモジュールの製造工程を説明するための図である。図7に示すように、まず、ヒートシンク10上にBステージ熱伝導性シート16を形成する(工程(a))。ここで、Bステージ熱伝導性シートは、上記熱硬化性樹脂組成物を用いてヒートシンク10上に直接形成することができる。或いは、別個にBステージ熱伝導性シート16を形成した後、Bステージ熱伝導性シート16をヒートシンク10上に配置してもよい。
次に、Bステージ熱伝導性シート16が形成されたヒートシンク10を、トランスファモールド用金型20内に配置する(工程(b))。
次に、電力半導体素子13及び金属線14を実装したリードフレーム12をBステージ熱伝導性シート16上に配置する(工程(c))。 Next, a method for manufacturing a power module having the above configuration will be described with reference to the drawings.
FIG. 7 is a diagram for explaining a manufacturing process of the power module of the present embodiment. As shown in FIG. 7, first, a B-stage thermally
Next, the
Next, the
最後に、トランスファモールド用金型20を除去することによって、パワーモジュールを得ることができる(工程(e))。
なお、得られたパワーモジュールは、必要に応じてポストキュアを行ってもよい。 Next, the sealing
Finally, the power module can be obtained by removing the transfer mold 20 (step (e)).
In addition, you may post-cure the obtained power module as needed.
実施例及び比較例で用いた二次焼結粒子は、窒化ホウ素の一次粒子と、水溶性バインダと、水とを含むスラリーを用いてスプレードライを行った後、約2000℃で焼結させることにより作製した。ここで、二次焼結粒子の最大空隙径は、スラリー中の水の量を調節することによって制御した。また、二次焼結粒子の最大空隙径は、二次焼結粒子をエポキシ樹脂に埋封したサンプルを作製し、そのサンプルの断面を研磨して電子顕微鏡で数千倍に拡大した写真を数枚撮影した後、二次焼結粒子の空隙の最大径を実際に測定することによって求めた。 Hereinafter, although an Example and a comparative example demonstrate the detail of this invention, this invention is not limited by these.
The secondary sintered particles used in Examples and Comparative Examples are sintered at about 2000 ° C. after spray drying using a slurry containing primary particles of boron nitride, a water-soluble binder, and water. It was produced by. Here, the maximum void diameter of the secondary sintered particles was controlled by adjusting the amount of water in the slurry. The maximum pore size of the secondary sintered particles is a number of photographs obtained by preparing a sample in which the secondary sintered particles are embedded in an epoxy resin, polishing the cross section of the sample, and magnifying it several thousand times with an electron microscope. After taking a picture, the maximum diameter of the voids of the secondary sintered particles was actually measured.
液状のビスフェノールA型エポキシ樹脂(ジャパンエポキシレジン株式会社製エピコート828)100質量部と、硬化剤である1-シアノメチル-2-メチルイミダゾール(四国化成工業株式会社製キュアゾール2PN-CN)1質量部と、溶媒であるメチルエチルケトン78質量部とを混合した。その後、この混合物に、無機充填材として二次焼結粒子及び鱗片状窒化ホウ素の一次粒子を加えて予備混合した。ここで、無機充填材は、熱伝導性シートにおいて5~30μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が10体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が15体積%となるように加えた。続いて、この予備混合物を三本ロールにて混練することによって熱硬化性樹脂組成物を得た。
次に、この熱硬化性樹脂組成物を、厚さ105μmの銅箔上にドクターブレード法を用いて塗布した後、110℃で15分間の加熱乾燥処理を行い、厚さ200μmのBステージ熱伝導性シートを得た。
次に、銅箔上に形成されたBステージ熱伝導性シートをトランスファモールド用金型に配置した後、電力半導体素子及び金属線を実装したリードフレームをBステージ熱伝導性シート上に配置した。そして、トランスファモールド用金型内に封止樹脂を流し込んで加圧成形した。この加圧成形において、成形温度を180℃、成形圧力を10MPa、成形時間を90秒とした。続いて、トランスファモールド用金型を取り外した後、175℃で8時間、ポストキュアすることにより、パワーモジュールを得た。 Example 1
100 parts by mass of a liquid bisphenol A type epoxy resin (Epicoat 828 manufactured by Japan Epoxy Resin Co., Ltd.) and 1 part by mass of 1-cyanomethyl-2-methylimidazole (Curesol 2PN-CN manufactured by Shikoku Kasei Kogyo Co., Ltd.) And 78 parts by mass of methyl ethyl ketone as a solvent were mixed. Thereafter, secondary sintered particles and scaly boron nitride primary particles were added to the mixture as an inorganic filler and premixed. Here, the inorganic filler is a secondary sintered particle having a maximum void diameter of 5 to 30 μm (average particle diameter of 65 μm) in the heat conductive sheet and having a maximum void diameter of less than 0.1 μm. Sintered particles (average particle size: 65 μm) were added at 10% by volume, and primary particles of flaky boron nitride (average major axis: 30 μm) were added at 15% by volume. Then, the thermosetting resin composition was obtained by kneading this preliminary mixture with a three roll.
Next, this thermosetting resin composition was applied onto a 105 μm thick copper foil using a doctor blade method, followed by a heat drying treatment at 110 ° C. for 15 minutes, and a B stage heat conduction having a thickness of 200 μm. Sex sheet was obtained.
Next, after the B-stage heat conductive sheet formed on the copper foil was placed in a transfer mold, the lead frame on which the power semiconductor element and the metal wire were mounted was placed on the B-stage heat conductive sheet. Then, a sealing resin was poured into the transfer mold and pressure-molded. In this pressure molding, the molding temperature was 180 ° C., the molding pressure was 10 MPa, and the molding time was 90 seconds. Subsequently, after removing the transfer mold, post-curing was performed at 175 ° C. for 8 hours to obtain a power module.
メチルエチルケトンの配合量を125質量部としたこと、及び無機充填材として、熱伝導性シートにおいて5~30μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が20体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が25体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Example 2)
The blending amount of methyl ethyl ketone was 125 parts by mass, and as an inorganic filler, secondary sintered particles (average particle size of 65 μm) having a maximum void diameter of 5 to 30 μm in the heat conductive sheet were 5% by volume, and. Except that secondary sintered particles (average particle size 65 μm) having a maximum void diameter of less than 1 μm were added in an amount of 20% by volume, and primary particles of flaky boron nitride (average
メチルエチルケトンの配合量を125質量部としたこと、及び無機充填材として、熱伝導性シートにおいて50~80μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が20体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が25体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Example 3)
The blending amount of methyl ethyl ketone was 125 parts by mass, and as an inorganic filler, secondary sintered particles (average particle size of 65 μm) having a maximum void diameter of 50 to 80 μm in the heat conductive sheet were 5% by volume, and. Except that secondary sintered particles (average particle size 65 μm) having a maximum void diameter of less than 1 μm were added in an amount of 20% by volume, and primary particles of flaky boron nitride (average
メチルエチルケトンの配合量を125質量部としたこと、及び無機充填材として、熱伝導性シートにおいて5~30μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が10体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が15体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が25体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 Example 4
The blending amount of methyl ethyl ketone was 125 parts by mass, and as the inorganic filler, secondary sintered particles (average particle size of 65 μm) having a maximum void diameter of 5 to 30 μm in the thermally conductive sheet were 10% by volume, and 0.0. Except that the secondary sintered particles having a maximum void diameter of less than 1 μm (average particle diameter of 65 μm) are 15% by volume, and the primary particles of flaky boron nitride (average major axis of 30 μm) are 25% by volume, A thermosetting resin composition, a B-stage heat conductive sheet and a power module were obtained in the same manner as in Example 1.
メチルエチルケトンの配合量を125質量部としたこと、及び無機充填材として、熱伝導性シートにおいて5~30μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が20体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が25体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Example 5)
The blending amount of methyl ethyl ketone was 125 parts by mass, and as the inorganic filler, secondary sintered particles (average particle diameter of 65 μm) having a maximum void diameter of 5 to 30 μm in the heat conductive sheet were 20% by volume, and 0.0. Except that the secondary sintered particles having a maximum void diameter of less than 1 μm (average particle diameter of 65 μm) are 5% by volume, and the primary particles of flaky boron nitride (average major axis of 30 μm) are 25% by volume, A thermosetting resin composition, a B-stage heat conductive sheet and a power module were obtained in the same manner as in Example 1.
メチルエチルケトンの配合量を234質量部としたこと、及び無機充填材として、熱伝導性シートにおいて5~30μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が30体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が35体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Example 6)
The blending amount of methyl ethyl ketone was 234 parts by mass, and as the inorganic filler, secondary sintered particles (average particle size 65 μm) having a maximum void diameter of 5 to 30 μm in the heat conductive sheet were 5% by volume, and 0.0. Except that secondary sintered particles (average particle size 65 μm) having a maximum void diameter of less than 1 μm were added to 30% by volume, and primary particles of flaky boron nitride (average
メチルエチルケトンの配合量を78質量部としたこと、及び無機充填材として、熱伝導性シートにおいて0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が15体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が15体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Comparative Example 1)
The blending amount of methyl ethyl ketone was 78 parts by mass, and as an inorganic filler, secondary sintered particles (average particle size 65 μm) having a maximum void diameter of less than 0.1 μm in the heat conductive sheet were 15% by volume, scaly A thermosetting resin composition, a B-stage thermal conductive sheet, and a power module were obtained in the same manner as in Example 1 except that the primary particles (average major axis: 30 μm) in the shape of boron nitride were added so as to be 15% by volume. It was.
メチルエチルケトンの配合量を125質量部としたこと、及び無機充填材として、熱伝導性シートにおいて0.1~1μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が20体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が25体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Comparative Example 2)
The blending amount of methyl ethyl ketone was 125 parts by mass, and as an inorganic filler, secondary sintered particles (average particle size 65 μm) having a maximum void diameter of 0.1 to 1 μm in the heat conductive sheet were 5% by volume, Other than adding secondary sintered particles (average particle size 65 μm) having a maximum void diameter of less than 0.1 μm to 20% by volume, and primary particles of flaky boron nitride (average
メチルエチルケトンの配合量を125質量部としたこと、及び無機充填材として、熱伝導性シートにおいて100~150μmの最大空隙径を有する二次焼結粒子(平均粒径65μm)が5体積%、0.1μm未満の最大空隙径を有する二次焼結粒子(平均粒径65μm)が20体積%、鱗片状窒化ホウ素の一次粒子(平均長径30μm)が25体積%となるように加えたこと以外は、実施例1と同様にして熱硬化性樹脂組成物、Bステージ熱伝導性シート及びパワーモジュールを得た。 (Comparative Example 3)
The blending amount of methyl ethyl ketone was 125 parts by mass, and as an inorganic filler, secondary sintered particles (average particle size of 65 μm) having a maximum void diameter of 100 to 150 μm in the heat conductive sheet were 5% by volume, and 0.0. Except that secondary sintered particles (average particle size 65 μm) having a maximum void diameter of less than 1 μm were added in an amount of 20% by volume, and primary particles of flaky boron nitride (average
これに対して比較例1のパワーモジュールに組み込まれた熱伝導性シートは、部分放電開始電圧及び絶縁破壊電圧の両方が低く、電気絶縁性が十分でなかった。この熱伝導性シートについて電子顕微鏡にて断面観察を行ったところ、熱伝導性シート内のベース部分や二次焼結粒子との界面部分に5μm以上の欠陥が発生していることを確認した。
同様に、比較例2のパワーモジュールに組み込まれた熱伝導性シートも、部分放電開始電圧及び絶縁破壊電圧の両方が低く、電気絶縁性が十分でなかった。この熱伝導性シートについて電子顕微鏡にて断面観察を行ったところ、熱伝導性シート内のベース部分や二次焼結粒子との界面部分、二次焼結粒子内の空隙部分などの様々な部分に欠陥が発生していることを確認した。
また、比較例3のパワーモジュールに組み込まれた熱伝導性シートは、部分放電開始電圧が低く、電気絶縁性が十分でなかった。この熱伝導性シートについて電子顕微鏡にて断面観察を行ったところ、熱伝導性シート内の欠陥は二次焼結粒子内の空隙部分に発生していたものの、欠陥の大きさが100μmを超えていることを確認した。 As can be seen from the results in Table 1, the thermal conductive sheets incorporated in the power modules of Examples 1 to 6 had both high partial discharge start voltage and dielectric breakdown voltage and good electrical insulation. When these cross sections of the heat conductive sheets were observed with an electron microscope, it was confirmed that defects in the heat conductive sheets were generated in void portions in the secondary sintered particles.
On the other hand, the heat conductive sheet incorporated in the power module of Comparative Example 1 had low partial discharge start voltage and dielectric breakdown voltage, and electrical insulation was not sufficient. When the cross section of this heat conductive sheet was observed with an electron microscope, it was confirmed that a defect of 5 μm or more was generated in the base part in the heat conductive sheet or the interface part with the secondary sintered particles.
Similarly, the heat conductive sheet incorporated in the power module of Comparative Example 2 also had low partial discharge start voltage and dielectric breakdown voltage, and electrical insulation was not sufficient. When this cross section of the thermally conductive sheet was observed with an electron microscope, various parts such as a base portion in the thermally conductive sheet, an interface portion with the secondary sintered particles, and a void portion in the secondary sintered particles It was confirmed that a defect occurred.
Moreover, the heat conductive sheet incorporated in the power module of Comparative Example 3 had a low partial discharge start voltage and insufficient electrical insulation. When the cross section of this thermally conductive sheet was observed with an electron microscope, defects in the thermally conductive sheet were generated in the voids in the secondary sintered particles, but the size of the defect exceeded 100 μm. I confirmed.
この実験で用いた二次焼結粒子は、平均長径3μmの窒化ホウ素の一次粒子と、水溶性バインダと、水とを含むスラリーを用いてスプレードライを行った後、約2,000℃で焼成して焼結(粒成長)させることによって作製した。ここで、一次粒子の平均長径は、二次焼結粒子をエポキシ樹脂に埋封したサンプルを作製し、そのサンプルの断面を研磨して電子顕微鏡で数千倍に拡大した写真を数枚撮影した後、一次粒子の長径を実際に測定し、その測定値を平均することによって求めた。
以下の実験で用いた密着性付与剤の種類及びその特性を表2に示す。 Next, the following experiment was performed in order to confirm the effect by mix | blending a specific adhesiveness imparting agent with a thermosetting resin composition.
The secondary sintered particles used in this experiment were spray dried using a slurry containing primary particles of boron nitride having an average major axis of 3 μm, a water-soluble binder, and water, and then fired at about 2,000 ° C. And then sintered (grain growth). Here, the average major axis of the primary particles was prepared by preparing a sample in which secondary sintered particles were embedded in an epoxy resin, and taking several photographs that were magnified several thousand times with an electron microscope by polishing the cross section of the sample. Thereafter, the major axis of the primary particles was actually measured, and the measured value was averaged.
Table 2 shows the types and characteristics of the adhesion-imparting agents used in the following experiments.
密着性付与剤A-1:19質量部と、メチルエチルケトンMEK(溶剤):181質量部とを攪拌混合した後、常温で固形のナフタレン型エポキシ樹脂(EPICLON EXA-4710:DIC株式会社製):80質量部、常温で液状のビスフェノールA型エポキシ樹脂(JER828:ジャパンエポキシレジン株式会社製):20質量部、及び1-シアノエチル-2-メチルイミダゾール(硬化剤、キュアゾール2PN-CN:四国化成工業株式会社製):1質量部を添加してさらに攪拌混合した。次に、この混合物に、上記で作製した窒化ホウ素の二次焼結粒子を、溶剤を除いた全成分の合計体積に対して40体積%となるように添加して予備混合した。この予備混合物を三本ロールにてさらに混練し、窒化ホウ素の二次焼結粒子が均一に分散された熱硬化性樹脂組成物を得た。 (Experiment 1)
Adhesion imparting agent A-1: 19 parts by mass and methyl ethyl ketone MEK (solvent): 181 parts by mass were stirred and mixed, and then a naphthalene type epoxy resin solid at room temperature (EPICLON EXA-4710: manufactured by DIC Corporation): 80 Bisphenol A type epoxy resin (JER828: manufactured by Japan Epoxy Resin Co., Ltd.): 20 parts by mass and 1-cyanoethyl-2-methylimidazole (curing agent, Curesol 2PN-CN: Shikoku Chemical Industry Co., Ltd.) (Product made): 1 part by mass was added and further stirred and mixed. Next, the boron nitride secondary sintered particles prepared above were added to this mixture so as to be 40% by volume with respect to the total volume of all components excluding the solvent, and premixed. This preliminary mixture was further kneaded with a three-roll to obtain a thermosetting resin composition in which secondary sintered particles of boron nitride were uniformly dispersed.
密着性付与剤A-1の代わりに密着性付与剤A-2を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験3)
密着性付与剤A-1の代わりに密着性付与剤A-3を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験4)
密着性付与剤A-1の代わりに密着性付与剤A-5を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。 (Experiment 2)
A thermosetting resin composition was obtained in the same manner as in
(Experiment 3)
A thermosetting resin composition was obtained in the same manner as in
(Experiment 4)
A thermosetting resin composition was obtained in the same manner as in
密着性付与剤A-1の代わりに密着性付与剤A-6を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験6)
密着性付与剤A-1:19質量部の代わりに密着性付与剤A-3:5質量部を用い、メチルエチルケトンMEKの添加量を160質量部に変えたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験7)
密着性付与剤A-1:19質量部の代わりに密着性付与剤A-3:11質量部を用い、メチルエチルケトンMEKの添加量を169質量部に変えたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。 (Experiment 5)
A thermosetting resin composition was obtained in the same manner as in
(Experiment 6)
Adhesion imparting agent A-1: Heat was applied in the same manner as in
(Experiment 7)
Adhesion imparting agent A-1: Heat was applied in the same manner as in
密着性付与剤A-1:19質量部の代わりに密着性付与剤A-3:25質量部を用い、メチルエチルケトンMEKの添加量を190質量部に変えたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験9)
密着性付与剤A-1の代わりに密着性付与剤A-8を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験10)
密着性付与剤A-1の代わりに密着性付与剤A-9を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(実験11)
密着性付与剤A-1の代わりに密着性付与剤A-3を用い、常温で固形のナフタレン型エポキシ樹脂(EPICLON EXA-4710:DIC株式会社製)の代わりに常温で固形のビフェニル型エポキシ樹脂(YX4000:ジャパンエポキシレジン株式会社製)を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。 (Experiment 8)
Adhesion imparting agent A-1: Heat was applied in the same manner as in
(Experiment 9)
A thermosetting resin composition was obtained in the same manner as in
(Experiment 10)
A thermosetting resin composition was obtained in the same manner as in
(Experiment 11)
Biphenyl type epoxy resin that is solid at room temperature instead of naphthalene type epoxy resin (EPICLON EXA-4710: manufactured by DIC Corporation) that is solid at room temperature by using adhesion agent A-3 instead of adhesion agent A-1. A thermosetting resin composition was obtained in the same manner as in
常温で固形のナフタレン型エポキシ樹脂(EPICLON EXA-4710:DIC株式会社製):80質量部、常温で液状のビスフェノールA型エポキシ樹脂(JER828:ジャパンエポキシレジン株式会社製):20質量部、1-シアノエチル-2-メチルイミダゾール(硬化剤、キュアゾール2PN-CN:四国化成工業株式会社製):1質量部、及びメチルエチルケトンMEK(溶剤):152質量部を攪拌混合した。次に、この混合物に、上記で作製した窒化ホウ素の二次焼結粒子を、溶剤を除いた全成分の合計体積に対して40体積%となるように添加して予備混合した。この予備混合物を三本ロールにてさらに混練し、窒化ホウ素の二次焼結粒子が均一に分散された熱硬化性樹脂組成物を得た。 (Comparative Experiment 1)
Naphthalene type epoxy resin solid at normal temperature (EPICLON EXA-4710: manufactured by DIC Corporation): 80 parts by mass, bisphenol A type epoxy resin liquid at normal temperature (JER828: manufactured by Japan Epoxy Resin Co., Ltd.): 20 parts by mass, 1- Cyanoethyl-2-methylimidazole (curing agent, Curazole 2PN-CN: manufactured by Shikoku Kasei Kogyo Co., Ltd.): 1 part by mass and methyl ethyl ketone MEK (solvent): 152 parts by mass were mixed with stirring. Next, the boron nitride secondary sintered particles prepared above were added to this mixture so as to be 40% by volume with respect to the total volume of all components excluding the solvent, and premixed. This preliminary mixture was further kneaded with a three-roll to obtain a thermosetting resin composition in which secondary sintered particles of boron nitride were uniformly dispersed.
密着性付与剤A-1の代わりに密着性付与剤A-4を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(比較実験3)
密着性付与剤A-1の代わりに密着性付与剤A-7を用いたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。 (Comparative experiment 2)
A thermosetting resin composition was obtained in the same manner as in
(Comparative Experiment 3)
A thermosetting resin composition was obtained in the same manner as in
密着性付与剤A-1:19質量部の代わりに密着性付与剤A-3:3質量部を用い、メチルエチルケトンMEKの添加量を157質量部に変えたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。
(比較実験5)
密着性付与剤A-1:19質量部の代わりに密着性付与剤A-3:34質量部を用い、メチルエチルケトンMEKの添加量を203質量部に変えたこと以外は実験1と同様にして熱硬化性樹脂組成物を得た。 (Comparative Experiment 4)
Adhesion imparting agent A-1: Heat was applied in the same manner as in
(Comparative Experiment 5)
Adhesion imparting agent A-1: Heat was applied in the same manner as in
次に、放熱部材上に形成した塗布乾燥物を、塗布乾燥物側が内側になるように2枚重ねた後、5MPaのプレス圧で加圧しながら120℃で20分間加熱することで半硬化(Bステージ)熱伝導性シートを得た。これをさらに5MPaのプレス圧で加圧しながら160℃で3時間加熱することで、Bステージ熱伝導性シートを完全に硬化させ、2つの放熱部材に挟まれた熱伝導性シート(厚さ200μm)を得た。 Each of the thermosetting resin compositions obtained in
Next, two sheets of the coated dried product formed on the heat radiating member are stacked so that the coated dried product side is inside, and then semi-cured by heating at 120 ° C. for 20 minutes while applying a pressurization pressure of 5 MPa (B Stage) A thermally conductive sheet was obtained. The B-stage heat conductive sheet is completely cured by heating at 160 ° C. for 3 hours while further pressurizing it with a press pressure of 5 MPa, and the heat conductive sheet (thickness 200 μm) sandwiched between two heat radiating members. Got.
なお、表3では、各実験及び比較実験で使用した構成成分の種類及び配合量についてもまとめた。各構成成分の配合量は質量部である。 Further, a thermally conductive sheet (thickness: 200 μm) was obtained in the same manner as described above except that the release-treated film was used in place of the heat radiating member, and the coated dried product was completely cured and then the film was removed. . About this heat conductive sheet, the glass transition temperature was measured using the dynamic viscoelasticity measuring apparatus. The results are shown in Table 3.
Table 3 also summarizes the types and blending amounts of the components used in each experiment and comparative experiment. The amount of each component is part by mass.
これに対して、密着性付与剤を配合しない熱硬化性樹脂組成物(比較実験1)、重量平均分子量又はガラス転移温度が所定の範囲にない可撓性樹脂を密着性付与剤として配合した熱硬化性樹脂組成物(比較実験2及び3)、密着性付与剤の配合量が適切でない熱硬化性樹脂組成物(比較実験4及び5)では、耐熱性は十分であったものの、熱伝導性、絶縁破壊電圧及び曲げ強度のいずれかが十分でなかった。
In contrast, a thermosetting resin composition that does not contain an adhesion-imparting agent (Comparative Experiment 1), a heat that contains a flexible resin whose weight average molecular weight or glass transition temperature is not within a predetermined range as an adhesion-imparting agent. In the curable resin composition (
図8からわかるように、密着性付与剤の配合量が5質量部以上30質量部以下の範囲にあると、十分な曲げ強度が得られ、熱伝導性シートの製造時(特に、Bステージ状態での成形・加工時)のハンドリング性が向上する。加えて、密着性付与剤の配合量がこの範囲にあると、絶縁破壊電圧が高くなる。逆に、密着性付与剤の配合量が5質量部以上30質量部以下の範囲にないと、十分な曲げ強度が得られず、熱伝導性シートの製造時(特に、Bステージ状態での成形・加工時)に割れや欠けが生じ、ハンドリング性が低下する。加えて、密着性付与剤の配合量がこの範囲にないと、絶縁破壊電圧も低くなる。 In order to examine these results in detail, the amount of adhesion imparting agent in
As can be seen from FIG. 8, when the blending amount of the adhesion-imparting agent is in the range of 5 parts by mass or more and 30 parts by mass or less, sufficient bending strength can be obtained, and at the time of manufacturing the heat conductive sheet (particularly, B stage state Handling at the time of molding and processing in). In addition, when the blending amount of the adhesion imparting agent is within this range, the dielectric breakdown voltage is increased. Conversely, if the blending amount of the adhesion-imparting agent is not in the range of 5 parts by mass or more and 30 parts by mass or less, sufficient bending strength cannot be obtained, and the heat conductive sheet is manufactured (particularly, molding in the B stage state).・ During processing, cracks and chipping occur, resulting in poor handling. In addition, if the compounding amount of the adhesion-imparting agent is not within this range, the dielectric breakdown voltage is also lowered.
このパワーモジュールにおいて、リードフレームと銅のヒートシンクの中央部とに熱電対を取り付けた後、パワーモジュールを稼動させ、リードフレームとヒートシンクとの温度をそれぞれ測定した。その結果、実施例1~11の熱硬化性樹脂組成物から得られた熱伝導性シートを用いたパワーモジュールはいずれも、リードフレームとヒートシンクとの温度差が小さく、熱放散性に優れていた。 Next, the heat conductive sheet obtained from the thermosetting resin composition of
In this power module, after attaching a thermocouple to the lead frame and the central part of the copper heat sink, the power module was operated and the temperatures of the lead frame and the heat sink were measured. As a result, all power modules using the heat conductive sheets obtained from the thermosetting resin compositions of Examples 1 to 11 had a small temperature difference between the lead frame and the heat sink and were excellent in heat dissipation. .
Claims (18)
- 無機充填材及び熱硬化性樹脂マトリックス成分を含む熱硬化性樹脂組成物であって、
前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有することを特徴とする熱硬化性樹脂組成物。 A thermosetting resin composition comprising an inorganic filler and a thermosetting resin matrix component,
The inorganic filler includes secondary sintered particles composed of primary particles of flaky boron nitride, and at least a part of the secondary sintered particles has a maximum void diameter of 5 μm or more and 80 μm or less. A thermosetting resin composition. - 前記二次焼結粒子の最大空隙径は、前記二次焼結粒子の平均粒径の2/3以下であることを特徴とする請求項1に記載の熱硬化性樹脂組成物。 The thermosetting resin composition according to claim 1, wherein the maximum void diameter of the secondary sintered particles is 2/3 or less of the average particle diameter of the secondary sintered particles.
- 前記無機充填材は、鱗片状窒化ホウ素の一次粒子をさらに含むことを特徴とする請求項1又は2に記載の熱硬化性樹脂組成物。 The thermosetting resin composition according to claim 1 or 2, wherein the inorganic filler further contains primary particles of scaly boron nitride.
- 600以上70,000以下の重量平均分子量及び130℃以下のガラス転移温度を有する可撓性樹脂である密着性付与剤を、熱硬化性樹脂マトリックス成分100質量部に対して5質量部以上30質量部以下の範囲でさらに含むことを特徴とする請求項1~3のいずれか一項に記載の熱硬化性樹脂組成物。 The adhesion-imparting agent, which is a flexible resin having a weight average molecular weight of 600 or more and 70,000 or less and a glass transition temperature of 130 ° C. or less, is 5 to 30 parts by mass with respect to 100 parts by mass of the thermosetting resin matrix component. The thermosetting resin composition according to any one of claims 1 to 3, further comprising:
- 前記可撓性樹脂は、ビスフェノール型エポキシ樹脂及びスチレン系ポリマーからなる群より選択される少なくとも1つであることを特徴とする請求項4に記載の熱硬化性樹脂組成物。 The thermosetting resin composition according to claim 4, wherein the flexible resin is at least one selected from the group consisting of a bisphenol type epoxy resin and a styrene polymer.
- 前記ビスフェノール型エポキシ樹脂は、以下の一般式(1)又は(2):
- 無機充填材をBステージ状態の熱硬化性樹脂マトリックス中に分散してなるBステージ熱伝導性シートであって、
前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有することを特徴とするBステージ熱伝導性シート。 A B-stage heat conductive sheet obtained by dispersing an inorganic filler in a B-stage thermosetting resin matrix,
The inorganic filler includes secondary sintered particles composed of primary particles of flaky boron nitride, and at least a part of the secondary sintered particles has a maximum void diameter of 5 μm or more and 80 μm or less. B-stage heat conductive sheet characterized. - 前記二次焼結粒子の最大空隙径は、前記二次焼結粒子の平均粒径の2/3以下であることを特徴とする請求項7に記載のBステージ熱伝導性シート。 The B-stage thermally conductive sheet according to claim 7, wherein the maximum pore size of the secondary sintered particles is 2/3 or less of the average particle size of the secondary sintered particles.
- 前記無機充填材は、鱗片状窒化ホウ素の一次粒子をさらに含むことを特徴とする請求項7又は8に記載のBステージ熱伝導性シート。 The B-stage heat conductive sheet according to claim 7 or 8, wherein the inorganic filler further contains primary particles of scaly boron nitride.
- 600以上70,000以下の重量平均分子量及び130℃以下のガラス転移温度を有する可撓性樹脂である密着性付与剤を、熱硬化性樹脂マトリックス100質量部に対して5質量部以上30質量部以下の範囲でさらに含むことを特徴とする請求項7~9のいずれか一項に記載のBステージ熱伝導性シート。 The adhesion imparting agent, which is a flexible resin having a weight average molecular weight of 600 or more and 70,000 or less and a glass transition temperature of 130 ° C. or less, is 5 parts by mass or more and 30 parts by mass with respect to 100 parts by mass of the thermosetting resin matrix. The B-stage heat conductive sheet according to any one of claims 7 to 9, further comprising the following range.
- 前記可撓性樹脂は、ビスフェノール型エポキシ樹脂及びスチレン系ポリマーからなる群より選択される少なくとも1つであることを特徴とする請求項10に記載のBステージ熱伝導性シート。 The B-stage heat conductive sheet according to claim 10, wherein the flexible resin is at least one selected from the group consisting of a bisphenol type epoxy resin and a styrene polymer.
- 前記ビスフェノール型エポキシ樹脂は、以下の一般式(1)又は(2):
- 無機充填材を熱硬化性樹脂マトリックス中に分散してなる熱伝導性シートであって、前記無機充填材は、鱗片状窒化ホウ素の一次粒子から構成される二次焼結粒子を含み、且つ前記二次焼結粒子の少なくとも一部が、5μm以上80μm以下の最大空隙径を有する熱伝導性シートを具備することを特徴とするパワーモジュール。 A thermally conductive sheet in which an inorganic filler is dispersed in a thermosetting resin matrix, wherein the inorganic filler includes secondary sintered particles composed of primary particles of scaly boron nitride, and At least a part of the secondary sintered particles includes a heat conductive sheet having a maximum void diameter of 5 μm or more and 80 μm or less.
- 前記二次焼結粒子の最大空隙径は、前記二次焼結粒子の平均粒径の2/3以下であることを特徴とする請求項13に記載のパワーモジュール。 The power module according to claim 13, wherein the maximum void diameter of the secondary sintered particles is 2/3 or less of the average particle diameter of the secondary sintered particles.
- 前記無機充填材は、鱗片状窒化ホウ素の一次粒子をさらに含むことを特徴とする請求項13又は14に記載のパワーモジュール。 The power module according to claim 13 or 14, wherein the inorganic filler further includes primary particles of scaly boron nitride.
- 前記熱伝導性シートは、600以上70,000以下の重量平均分子量及び130℃以下のガラス転移温度を有する可撓性樹脂である密着性付与剤を、熱硬化性樹脂マトリックス100質量部に対して5質量部以上30質量部以下の範囲でさらに含むことを特徴とする請求項13~15のいずれか一項に記載のパワーモジュール。 The heat conductive sheet is a flexible resin having a weight average molecular weight of 600 or more and 70,000 or less and a glass transition temperature of 130 ° C. or less, with respect to 100 parts by mass of the thermosetting resin matrix. The power module according to any one of claims 13 to 15, further comprising 5 to 30 parts by mass.
- 前記可撓性樹脂は、ビスフェノール型エポキシ樹脂及びスチレン系ポリマーからなる群より選択される少なくとも1つであることを特徴とする請求項16に記載のパワーモジュール。 The power module according to claim 16, wherein the flexible resin is at least one selected from the group consisting of a bisphenol type epoxy resin and a styrene polymer.
- 前記ビスフェノール型エポキシ樹脂は、以下の一般式(1)又は(2):
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Also Published As
Publication number | Publication date |
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CN102770956A (en) | 2012-11-07 |
JP5340202B2 (en) | 2013-11-13 |
CN102770956B (en) | 2015-04-29 |
US9029438B2 (en) | 2015-05-12 |
DE112010005303T5 (en) | 2012-12-20 |
JP2011176024A (en) | 2011-09-08 |
DE112010005303B4 (en) | 2016-07-07 |
US20130012621A1 (en) | 2013-01-10 |
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